Nitrogen, Ammonia, 8155

Nitrogen, Ammonia DOC316.53.01077

Salicylate Method1 Method 8155

0.01 to 0.50 mg/L NH3–N Powder Pillows
Scope and Application: For water, wastewater and seawater
1 Adapted from Clin. Chim. Acta., 14, 403 (1966)

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between
instruments. To use this table, select an instrument then read across to find the corresponding
information required to perform this test.

Table 258 Instrument-specific information

Instrument Sample cell Cell orientation

DR 6000 2495402 Fill line faces right

DR 5000 2495402 Fill line faces user

DR 3900 2495402 Fill line faces user

DR 3800, DR 2800, DR 2700 2495402 Fill line faces right

Before starting the test:

A green color will develop if ammonia nitrogen is present.

Dispose of reacted solutions according to local, state and federal regulations. Use the guidance given on the Material Safety
Data Sheets to dispose of unreacted reagents. Consult local regulatory agencies for further disposal information.

Collect the following items:

Description Quantity

Ammonia Cyanurate Reagent pillows 2

Ammonia Salicylate Reagent pillows 2

Sample Cells (see Instrument-specific information) 2

Stopper for sample cells 2

See Consumables and replacement items for reorder information.

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Salicylate method for powder pillows

Stored Programs

385 N, Ammonia, Salic

Start

1. Select the test. 2. Prepared Sample: 3. Blank Preparation: 4. Add the contents of
Insert an adapter if Fill a sample cell to the 10- Fill a second sample cell one Ammonia Salicylate
required (see Instrument- mL mark with sample. to the 10-mL mark with Powder Pillow to each cell.
specific information). deionized water.
Refer to the user manual
for orientation.

5. Insert the stopper or 6. Start the instrument
cap the cell and shake to timer.
dissolve. A three-minute reaction
period will begin.
7. When the timer 8. Stopper or cap and
expires, add the contents shake to dissolve.
of one Ammonia
Cyanurate Reagent
Powder Pillow to each cell.

Zero

9. Start the instrument 10. When the timer 11. ZERO the instrument. 12. Wipe the sample and
timer. expires, wipe the blank The display will show: insert it into the cell holder.
A 15-minute reaction and insert it into the cell 0.00 mg/L NH3–N. READ the results in mg/L
period will begin. holder NH3–N.
A green color will develop
if ammonia-nitrogen
is present.

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Interferences

Table 259 Interfering substances

Interfering substance Interference level
Calcium Greater than 1000 mg/L as CaCO3
All levels. Correct for iron interference as follows:
1. Determine the amount of iron present in the sample by following one of the Iron, Total,
Iron procedures.
2. Add the same iron concentration to the ammonia-free water in step 2. The interference
will be successfully blanked out.
Magnesium Greater than 6000 mg/L as CaCO3
Monochloramine present in chloraminated drinking water interferes directly at all levels,
Monochloramine giving high results. Use Method 10200, Free Ammonia and Monochloramine, to determine
free ammonia in these sample matrices.
Nitrate Greater than 100 mg/L as NO3––N
Nitrite Greater than 12 mg/L as NO2––N
Phosphate Greater than 100 mg/L as PO43––P
Sulfate Greater than 300 mg/L as SO42–
Sulfide will intensify the color. Eliminate sulfide interference as follows:
1. Measure about 350 mL of sample in a 500-mL Erlenmeyer flask1.
Sulfide 2. Add the contents of one Sulfide Inhibitor Reagent1 Powder Pillow. Swirl to mix.
3. Filter the sample through a Folded Filter Paper1 and Filter Funnel1.
4. Use the filtered solution in step 3.
Less common interferences such as hydrazine and glycine will cause intensified colors in
the prepared sample. Turbidity and color will give erroneous high values. Samples with
Other Substances
severe interferences require distillation. Use the distillation procedure with the General
Purpose Distillation Set.
1 See Optional reagents and apparatus.

Sample collection, preservation and storage

• Collect samples in clean plastic or glass bottles. Most reliable results are obtained when
samples are analyzed as soon as possible after collection.
• If chlorine is known to be present, add one drop of 0.1 N Sodium Thiosulfate* for each 0.3
mg/L Cl2 in a one-liter sample.
• Adjust the pH to 2 or less with concentrated (about 2 mL per liter) Sulfuric Acid.
• Store samples at 4 °C or less. Samples preserved in this manner can be stored up to 28 days.
• Just before testing the stored sample, warm to room temperature and neutralize with 5.0 N
Sodium Hydroxide Standard Solution.
• Correct the test result for volume additions.

* See Optional reagents and apparatus.

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Accuracy check
Standard additions method (sample spike)
Required for accuracy check:
• Ammonia Nitrogen Standard Solution, 10-mg/L as NH3–N
• TenSette Pipet and Pipet Tips
• 25-mL Mixing cylinders (3)

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.

2. Select standard additions from the instrument menu OPTIONS>MORE>STANDARD

ADDITIONS.

3. Accept the default values for standard concentration, sample volume and spike volumes. After
the values are accepted, the unspiked sample reading will appear in the top row. See the user
manual for more information.

4. Open the standard solution.

5. Use the TenSette Pipet to prepare spiked samples: add 0.2 mL, 0.4 mL and 0.6 mL of
standard to three 25-mL portions of fresh sample in three mixing cylinders.

6. Follow the Salicylate method for powder pillows test procedure for each of the spiked samples,
starting with the 0.2 mL sample spike. Measure each of the spiked samples in the instrument.

7. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.

Standard solution method

Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check:

• Ammonia Nitrogen Standard Solution, 10-mg/L as NH3–N
• TenSette Pipet, 0.1–1.0 mL and Pipet Tips

OR

• Ammonia Nitrogen Voluette® Standard Solution, 50-mg/L as NH3–N

• Deionized water
• 100 mL Class A volumetric flask
• 4-mL Class A volumetric pipet

1. Prepare a 0.40 mg/L ammonia nitrogen standard solution as follows:

• Dilute 4.00 mL of Ammonia Nitrogen Standard Solution, 10-mg/L to 100 mL with
deionized water.

OR

• Use the TenSette® Pipet to dilute 0.8 mL of an Ammonia Nitrogen Voluette Standard
Solution, 50-mg/L as NH3–N, to 100 mL with deionized water

2. Use the 0.40-mg/L solution in place of the sample. Follow the Salicylate method for powder
pillows test procedure.

3. To adjust the calibration curve using the reading obtained with the standard solution, navigate
to Standard Adjust in the software OPTIONS>MORE>STANDARD ADJUST.

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4. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate
concentration is used, enter the concentration and adjust the curve to that value.

Method performance

Precision—95% Confidence Sensitivity—ΔConcentration

Program Standard
Limits of Distribution per 0.010 ΔAbs
385 0.40 mg/L NH3–N 0.38–0.42 mg/L NH3–N 0.004 mg/L NH3–N

Summary of method
Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts
with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a
sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the
yellow color from the excess reagent present to give a final green-colored solution. Test results are
measured at 655 nm.

Consumables and replacement items

Required reagents
Description Quantity/Test Unit Catalog number
Ammonia Nitrogen Reagent Set for 10-mL samples (100 tests), — — 2668000
includes:
Includes:
(2) Ammonia Cyanurate Reagent Powder Pillows 2 100/pkg 2653199
(2) Ammonia Salicylate Reagent Powder Pillows 2 100/pkg 2653299

Recommended standards and apparatus

Description Unit Catalog number
Nitrogen, Ammonia Standard Solution, 10-mg/L NH3–N 500 mL 15349
Nitrogen, Ammonia Standard Solution, 10-mL Voluette® Ampule, 50-mg/L NH3–N 16/pkg 147910
Wastewater, Effluent Inorganics, for NH3–N, NO3–N, PO4, COD, SO4, TOC 500 mL 2833249
Pipet, TenSette® 0.1 - 1.0 mL each 1970001
Pipet Tips, for TenSette Pipet 1970001 50/pkg 2185696
Pipet Tips, for TenSette Pipet 1970001 1000/pkg 2185628
Flask, volumetric, Class A, 100 mL each 1457442
Pipet, volumetric, Class A, 4.00 mL each 1451504
Stopper, 18 mm each 6/pkg
Water, deionized 4L 27256
Sample cell, 10 mL square, matched pair 2/pkg 2495402

Optional reagents and apparatus

Description Unit Catalog number
Cylinder, mixing, 25-mL each 2088640

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Optional reagents and apparatus

Description Unit Catalog number
Distillation Set, general purpose each 2265300
Erlenmeyer Flask, 500 mL each 50549
Filter Funnel, Analytical PP, 65 mm each 108367
Filter Paper, folded, 12.5 cm 100/pkg 189457
Heater and support apparatus; 115 Vac, 60 Hz each 2274400
Heater and support apparatus, 230 Vac, 50 Hz each 2274402
Pipet, 2 mL Serological each 53236
Ampule breaker, Voluette each 2196800
Sodium Hydroxide Standard Solution, 5.0 N 50 mL SCDB 245026
Sulfide Inhibitor Reagent Powder Pillow 100/pkg 241899
Sulfuric Acid, Conc 500 mL 97949

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